CN112023985A - Preparation method of composite nano photocatalytic material - Google Patents
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- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 22
- NVWBARWTDVQPJD-UHFFFAOYSA-N antimony(3+);trisulfide Chemical compound [S-2].[S-2].[S-2].[Sb+3].[Sb+3] NVWBARWTDVQPJD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229940007424 antimony trisulfide Drugs 0.000 claims abstract description 18
- 239000002121 nanofiber Substances 0.000 claims abstract description 15
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 claims abstract description 14
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 claims abstract description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011593 sulfur Substances 0.000 claims abstract description 9
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 235000019441 ethanol Nutrition 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 10
- 239000007795 chemical reaction product Substances 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 5
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 5
- IHBMMJGTJFPEQY-UHFFFAOYSA-N sulfanylidene(sulfanylidenestibanylsulfanyl)stibane Chemical compound S=[Sb]S[Sb]=S IHBMMJGTJFPEQY-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- PWKSKIMOESPYIA-UHFFFAOYSA-N 2-acetamido-3-sulfanylpropanoic acid Chemical group CC(=O)NC(CS)C(O)=O PWKSKIMOESPYIA-UHFFFAOYSA-N 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 2
- 239000012876 carrier material Substances 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 238000013032 photocatalytic reaction Methods 0.000 abstract description 2
- 238000004729 solvothermal method Methods 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 1
- -1 polytetrafluoroethylene Polymers 0.000 abstract 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 1
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 1
- 229910001220 stainless steel Inorganic materials 0.000 abstract 1
- 239000010935 stainless steel Substances 0.000 abstract 1
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- 239000011941 photocatalyst Substances 0.000 description 6
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 235000013878 L-cysteine Nutrition 0.000 description 2
- 239000004201 L-cysteine Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/34—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of chromium, molybdenum or tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention provides a preparation method of a composite nano photocatalytic material, belonging to the field of photocatalysis. The preparation method comprises the following preparation steps: 1) successively dissolving a certain amount of ammonium tetrathiomolybdate and antimony trichloride in absolute ethyl alcohol, stirring and fully dissolving, continuously adding polyacrylonitrile nano-fiber serving as a carrier into the absolute ethyl alcohol solution, and slowly dripping the absolute ethyl alcohol solution containing a certain amount of sulfur source into the solution to obtain a precursor solution; 2) putting the precursor solution obtained in the step 1) into a sealed stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, and putting the reaction kettle into a constant-temperature oven for high-temperature reaction; 3) and (3) cleaning the product in the reaction kettle in the step 2) by using ethanol and deionized water in sequence, and drying in vacuum to obtain the antimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano material. The invention has the remarkable characteristics that: 1) the one-step solvothermal method is adopted, so that the preparation method is simple, easy to recover, low in cost and low in energy consumption; 2) the polyacrylonitrile nano-fiber is used as a carrier, which is beneficial to the stability and dispersion of nano-particles, increases active sites for reaction and is beneficial to the implementation of photocatalytic reaction; 3) the composite material effectively avoids the combination of semiconductor photoproduction electrons and cavities, and improves the degradation efficiency of the photocatalytic material.
Description
Technical Field
The invention relates to a preparation method of a composite nano photocatalytic material, belonging to the field of photocatalysis.
Background
With the rapid development of economic society, the problem of treating organic pollutants in wastewater is not easy. Among the numerous water treatment processes, photocatalytic technology is one of the hot spots in research. In recent years, many semiconductor photocatalysts are researched, and besides common materials such as zinc oxide and titanium dioxide, sulfides such as antimony trisulfide and molybdenum dioxide are considered to be ideal photocatalysts at present. The main disadvantage of antimony trisulfide is that photo-generated electron-hole pairs are easily recombined and the electron transfer rate is slow. Molybdenum disulfide as a two-dimensional layered material similar to graphene has more active sites, so that the molybdenum disulfide has certain adsorption performance and provides possibility for rapid migration of electrons. If the molybdenum disulfide and the antimony trisulfide form a composite material, the carrier migration rate of the antimony trisulfide is improved, the recombination of photo-generated electrons and holes is effectively inhibited, and the photocatalytic efficiency is improved.
The polyacrylonitrile nano-fiber is used as a carrier, which is beneficial to the stability and dispersion of nano-particles, increases active sites for reaction and is beneficial to the implementation of photocatalytic reaction. In a word, antimony trisulfide and molybdenum disulfide nano structures are loaded on polyacrylonitrile nano fibers, so that the photocatalytic performance and the reusability are improved by utilizing respective advantages and synergistic effects of the antimony trisulfide and the molybdenum disulfide nano structures.
Disclosure of Invention
The invention aims to provide a preparation method of a visible light response composite nano photocatalytic material, which solves the problems of high cost, difficult reutilization and low degradation efficiency of the existing deep purification of organic pollutants in wastewater. The composite material adopts a one-step solvothermal method, and has the advantages of simple preparation method, low cost, low energy consumption, higher degradation efficiency and reusability.
A preparation method of a composite nano photocatalytic material is characterized by comprising the following steps:
1) successively dissolving a certain amount of ammonium tetrathiomolybdate and antimony trichloride in 40mL of absolute ethanol, magnetically stirring to fully dissolve the ammonium tetrathiomolybdate and the antimony trichloride, and simultaneously dispersing and adding a certain mass of polyacrylonitrile nano fibers into the ethanol solution to obtain a mixed solution;
2) dissolving a certain amount of sulfur source in 10mL of absolute ethyl alcohol, slowly dripping the sulfur source into the mixed solution obtained in the step 1) after magnetic stirring to obtain a precursor solution;
3) putting the precursor solution in the step 2) into a reaction kettle, and reacting for a certain time at a certain temperature;
4) and (3) naturally cooling the reaction kettle in the step 3) to room temperature, taking out a reaction product in the kettle, sequentially washing the reaction product with ethanol and deionized water for 3 times, and drying the reaction product in vacuum at the temperature of 60 ℃ for 8 hours to obtain the product of the diantimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano photocatalytic material.
According to the scheme, the mass of the polyacrylonitrile nano-fiber is 0.02-0.05 g.
According to the scheme, the mass ratio of antimony trichloride to ammonium tetrathiomolybdate (3-6): 1.
according to the scheme, the quantity ratio of antimony trichloride to sulfur source substances is 1: (2-7).
According to the scheme, the sulfur source is L-cysteine, thiourea, thioacetamide or sodium sulfide.
According to the scheme, the reaction temperature of the reaction kettle is 160-200 ℃, and the heating reaction time is 8-15 hours.
The working principle of the invention is as follows: the polyacrylonitrile nano-fiber is used as a carrier, molybdenum disulfide and antimony trisulfide which are narrow-band gap semiconductor materials are compounded to obtain a novel stable visible light catalytic material, and due to the matched conduction band and valence band positions, the recombination probability of photo-generated electrons and holes is effectively reduced, the survival time of the photo-generated electrons is prolonged, and the photocatalytic performance is improved.
The invention has the following beneficial effects:
the invention is synthesized by a one-step solvent thermal method, has simple operation, cheap and easily obtained raw materials and low cost, and the prepared material has better photocatalytic performance and can be repeatedly utilized. Has wide application prospect in the fields of environmental monitoring and treatment and material chemistry.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of the antimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano photocatalytic material prepared in example 1;
FIG. 2 is an X-ray powder diffraction (XRD) spectrum of the antimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano photocatalytic material prepared in example 1;
FIG. 3 is a graph of the ultraviolet-visible diffuse reflection (UV-Vis DRS) spectrum of the antimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano photocatalytic material prepared in example 1;
FIG. 4 (A) is a graph showing the change of absorption spectrum of methylene blue solution degraded by antimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano material prepared in example 1 as photocatalyst under the action of visible light; fig. 4 (B) is a graph showing the change of the degradation efficiency of the antimony trisulfide/molybdenum disulfide/polyacrylonitrile composite material prepared in example 1 to the methylene blue solution with the reaction time under the action of visible light, and in addition, the change of the degradation efficiency of the antimony trisulfide/polyacrylonitrile and the molybdenum disulfide/polyacrylonitrile to the methylene blue solution with the reaction time is used as a comparison.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
Example 1:
1) sequentially dissolving 0.15mmol of ammonium tetrathiomolybdate and 0.6mmol of antimony trichloride in 40mL of absolute ethanol, magnetically stirring for 1 hour to fully dissolve the ammonium tetrathiomolybdate and the antimony trichloride, and simultaneously dispersing and adding 0.03g of polyacrylonitrile nano fibers into the ethanol solution to obtain a mixed solution;
2) dissolving 1.3mmol of L-cysteine in 10mL of absolute ethyl alcohol, and slowly dripping the solution into the mixed solution in the step 1) after magnetic stirring to obtain a precursor solution;
3) putting the precursor solution in the step 2) into a reaction kettle, and heating for 10 hours at 180 ℃;
4) and (3) naturally cooling the reaction kettle in the step 3) to room temperature, taking out a reaction product in the kettle, sequentially washing the reaction product with ethanol and deionized water for 3 times, and drying the reaction product in vacuum at the temperature of 60 ℃ for 8 hours to obtain the product of the diantimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano photocatalytic material.
Example 2:
this example differs from example 1 in that: 0.45mmol of antimony trichloride is added in the step 1). The rest is the same as in embodiment 1.
Example 3:
this example differs from example 1 in that: step 2) 3mmol of L-cysteine was added. The rest is the same as in embodiment 1.
Example 4:
this example differs from example 1 in that: 0.05g of polyacrylonitrile nano-fiber is added in the step 1). The rest is the same as in embodiment 1.
Example 5:
this example differs from example 1 in that: step 2) 1.3mmol of sodium sulfide was added. The rest is the same as in embodiment 1.
Example 6:
this example differs from example 1 in that: in step 2) 4mmol of sodium sulfide was added. The rest is the same as in embodiment 1.
Example 7:
this example differs from example 1 in that: the reaction temperature of the reaction kettle in the step 3) is 180 ℃, and the heating reaction time is 15 h. The rest is the same as in embodiment 1.
Example 8:
this example differs from example 1 in that: adding 0.9mmol of antimony trichloride into the step 1); step 2) was followed by the addition of 3.6mmol of sodium sulfide. The rest is the same as in embodiment 1.
Example 9:
this example differs from example 1 in that: adding 0.05g of polyacrylonitrile nano fiber in the step 1), wherein the reaction temperature of the reaction kettle in the step 3) is 200 ℃, and the heating reaction time is 14 h. The rest is the same as in embodiment 1.
Example 10:
this example differs from example 1 in that: adding 0.35mmol of antimony trichloride into the step 1); 0.045g polyacrylonitrile nanofibers; adding 2.1mmol of thiourea into the step 2); the reaction temperature of the reaction kettle in the step 3) is 160 ℃, and the heating reaction time is 8 h. The rest is the same as in embodiment 1.
The antimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano material prepared in example 1 is used as a photocatalyst to degrade methylene blue solution. 0.03g of photocatalyst was added to 50mL of a methylene blue solution having a concentration of 10mg/L, and a 350W xenon lamp was used as a light source. And 5mL of supernatant of the methylene blue solution is taken every 30min, the supernatant is measured by an ultraviolet spectrophotometer after centrifugal separation, and the concentration change of the methylene blue in the photodegradation process is determined according to the light absorption value of 664 nm. Experimental results show that the methylene blue solution added with the diantimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano photocatalyst is basically and completely degraded after being illuminated for 150 min. Therefore, the antimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano material prepared by the method has high-efficiency photocatalytic performance.
The above description is only a preferred and representative embodiment of the present invention, and the upper and lower limit values and interval values of each raw material and process mode can implement the present invention, and the examples are not listed here.
Claims (7)
1. A preparation method of a composite nano photocatalytic material is characterized in that molybdenum disulfide and antimony trisulfide are used as catalytic active components, polyacrylonitrile nano-fibers are used as carrier materials, and the molybdenum disulfide and the antimony trisulfide are stably dispersed on the polyacrylonitrile nano-fibers.
2. A preparation method of the antimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano photocatalytic material as claimed in claim 1 is characterized by comprising the following steps:
1) successively dissolving a certain amount of ammonium tetrathiomolybdate and antimony trichloride in 40mL of absolute ethanol, magnetically stirring to fully dissolve the ammonium tetrathiomolybdate and the antimony trichloride, and simultaneously dispersing and adding a certain mass of polyacrylonitrile nano fibers into the ethanol solution to obtain a mixed solution;
2) dissolving a certain amount of sulfur source in 10mL of absolute ethyl alcohol, slowly dripping the sulfur source into the mixed solution obtained in the step 1) after magnetic stirring to obtain a precursor solution;
3) putting the precursor solution in the step 2) into a reaction kettle, and reacting for a certain time at a certain temperature;
4) and (3) naturally cooling the reaction kettle in the step 3) to room temperature, taking out a reaction product in the kettle, sequentially washing the reaction product with ethanol and deionized water for 3 times, and drying the reaction product in vacuum at the temperature of 60 ℃ for 8 hours to obtain the product of the diantimony trisulfide/molybdenum disulfide/polyacrylonitrile composite nano photocatalytic material.
3. The method of claim 2, wherein: the mass of the polyacrylonitrile nano-fiber in the step 1) is 0.02-0.05 g.
4. The method of claim 2, wherein: the mass ratio of antimony trichloride to ammonium tetrathiomolybdate in the step 1) (3-6): 1.
5. the method of claim 2, wherein: the mass ratio of the antimony trichloride in the step 1) to the sulfur source substance in the step 2) is 1: (2-7).
6. The method of claim 2, wherein: in the step 2), the sulfur source is L-cysteine, thiourea, thioacetamide or sodium sulfide.
7. The method of claim 2, wherein: the reaction temperature of the reaction kettle in the step 3) is 160-200 ℃, and the heating reaction time is 8-15 h.
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| CN115888818A (en) * | 2022-07-29 | 2023-04-04 | 南京工业大学 | Micro-fluidic electrostatic spinning in-situ growth flue gas denitration catalyst and preparation method and application thereof |
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